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#$Date: 2021-12-06 10:59:38 +0200 (Mon, 06 Dec 2021) $
#$Revision: 271126 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/55/1565550.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1565550
loop_
_publ_author_name
'López Plá, Jessica M.'
'Boudalis, Athanassios K.'
'Telser, Joshua'
'Raptis, Raphael G.'
_publ_section_title
;
 Chromium(III)-pyrazole complexes. X-Ray crystal structures, 1H NMR
 investigation of ligand fluxional behavior and EPR studies
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119299
_journal_paper_doi               10.1016/j.ica.2019.119299
_journal_volume                  502
_journal_year                    2020
_chemical_formula_moiety         'C9 H9 Cl6 Cr N6'
_chemical_formula_sum            'C9 H9 Cl6 Cr N6'
_chemical_formula_weight         465.92
_chemical_name_systematic        mer-CrCl3(4-Cl-pzH)3
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_cell_angle_alpha                78.808(15)
_cell_angle_beta                 89.621(15)
_cell_angle_gamma                88.186(15)
_cell_formula_units_Z            2
_cell_length_a                   6.792(3)
_cell_length_b                   10.395(3)
_cell_length_c                   12.218(4)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    295.15
_cell_measurement_theta_max      30.08
_cell_measurement_theta_min      2.87
_cell_volume                     845.8(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      295.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16370
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.304
_diffrn_reflns_theta_min         2.864
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.626
_exptl_absorpt_correction_T_max  0.9014
_exptl_absorpt_correction_T_min  0.7824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0435 before and 0.0384 after correction. The Ratio of minimum to maximum transmission is 0.8680. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'clear grayish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   grayish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_description       cubic
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0292P)²+0.5222P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2900
_reflns_number_total             3424
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2020-502-119299.cif
_cod_data_source_block           jlp068_a
_cod_original_cell_volume        845.7(5)
_cod_database_code               1565550
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.738
_olex2_refinement_description
;
1. Others
 Fixed Sof: Cl5B(0.45) Cl5A(0.55)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.17052(5) 0.31946(3) 0.79506(3) 0.02681(9) Uani 1 1 d . . . . .
Cl1 Cl -0.06257(8) 0.44832(6) 0.67760(5) 0.04010(14) Uani 1 1 d . . . . .
Cl2 Cl -0.01599(9) 0.33902(6) 0.95136(5) 0.04356(15) Uani 1 1 d . . . . .
Cl3 Cl 0.41017(8) 0.18888(5) 0.89863(4) 0.03732(13) Uani 1 1 d . . . . .
Cl4 Cl 0.36767(9) 0.85104(6) 0.83611(5) 0.04714(16) Uani 1 1 d . . . . .
Cl5B Cl 0.7151(11) 0.1639(7) 0.4608(7) 0.0843(18) Uani 0.45 1 d . . P A 2
Cl6 Cl -0.16696(11) -0.14605(7) 0.66819(7) 0.0630(2) Uani 1 1 d . . . . .
N1 N 0.3222(2) 0.48516(17) 0.81155(14) 0.0313(4) Uani 1 1 d . . . . .
N2 N 0.5097(3) 0.4857(2) 0.84940(17) 0.0382(4) Uani 1 1 d . . . . .
H2 H 0.575(4) 0.416(3) 0.863(2) 0.041(7) Uiso 1 1 d . . . . .
N3 N 0.3334(2) 0.30287(17) 0.65074(14) 0.0303(4) Uani 1 1 d . . . . .
N4 N 0.2889(3) 0.3728(2) 0.54835(16) 0.0398(5) Uani 1 1 d . . . . .
H4 H 0.194(5) 0.424(3) 0.543(2) 0.059(9) Uiso 1 1 d . . . . .
N5 N 0.0204(2) 0.15174(17) 0.78300(14) 0.0316(4) Uani 1 1 d . . . . .
N6 N -0.0887(3) 0.0891(2) 0.86886(17) 0.0401(5) Uani 1 1 d . . . . .
H6 H -0.108(4) 0.122(3) 0.922(2) 0.055(9) Uiso 1 1 d . . . . .
C1 C 0.2530(3) 0.6083(2) 0.80312(19) 0.0343(5) Uani 1 1 d . . . . .
H1 H 0.129(4) 0.631(2) 0.7805(19) 0.036(6) Uiso 1 1 d . . . . .
C2 C 0.3963(3) 0.6860(2) 0.83456(18) 0.0337(5) Uani 1 1 d . . . . .
C3 C 0.5577(4) 0.6054(2) 0.8638(2) 0.0402(5) Uani 1 1 d . . . . .
H3 H 0.684(4) 0.621(3) 0.889(2) 0.055(8) Uiso 1 1 d . . . . .
C4 C 0.4933(4) 0.2315(3) 0.6346(2) 0.0464(6) Uani 1 1 d . . . . .
H4A H 0.543(4) 0.180(3) 0.687(2) 0.048(8) Uiso 1 1 d . . . . .
C5 C 0.5464(4) 0.2570(3) 0.52315(19) 0.0472(6) Uani 1 1 d . . . . .
C6 C 0.4149(4) 0.3468(3) 0.4704(2) 0.0439(6) Uani 1 1 d . . . . .
H6A H 0.410(4) 0.387(3) 0.402(2) 0.052(8) Uiso 1 1 d . . . . .
C7 C 0.0097(3) 0.0804(2) 0.7042(2) 0.0363(5) Uani 1 1 d . . . . .
H7 H 0.073(3) 0.101(2) 0.637(2) 0.036(6) Uiso 1 1 d . . . . .
C8 C -0.1085(3) -0.0268(2) 0.7409(2) 0.0368(5) Uani 1 1 d . . . . .
C9 C -0.1688(4) -0.0184(2) 0.8460(2) 0.0421(6) Uani 1 1 d . . . . .
H9 H -0.240(4) -0.070(3) 0.896(2) 0.046(7) Uiso 1 1 d . . . . .
Cl5A Cl 0.7600(9) 0.2081(6) 0.4637(6) 0.0736(12) Uani 0.55 1 d . . P A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Cl2 Cr1 Cl1 91.00(3) . .
Cl3 Cr1 Cl1 175.71(2) . .
Cl3 Cr1 Cl2 93.20(3) . .
N1 Cr1 Cl1 91.11(6) . .
N1 Cr1 Cl2 89.70(5) . .
N1 Cr1 Cl3 89.77(6) . .
N1 Cr1 N3 90.85(7) . .
N3 Cr1 Cl1 87.67(5) . .
N3 Cr1 Cl2 178.57(5) . .
N3 Cr1 Cl3 88.12(5) . .
N5 Cr1 Cl1 90.09(6) . .
N5 Cr1 Cl2 89.35(5) . .
N5 Cr1 Cl3 89.10(6) . .
N5 Cr1 N1 178.48(7) . .
N5 Cr1 N3 90.13(7) . .
N2 N1 Cr1 125.61(14) . .
C1 N1 Cr1 128.59(15) . .
C1 N1 N2 105.20(18) . .
N1 N2 H2 118.9(18) . .
C3 N2 N1 111.51(19) . .
C3 N2 H2 129.5(18) . .
N4 N3 Cr1 123.25(14) . .
C4 N3 Cr1 132.39(15) . .
C4 N3 N4 104.36(18) . .
N3 N4 H4 118(2) . .
C6 N4 N3 112.3(2) . .
C6 N4 H4 130(2) . .
N6 N5 Cr1 121.21(14) . .
C7 N5 Cr1 133.26(15) . .
C7 N5 N6 105.48(18) . .
N5 N6 H6 120(2) . .
C9 N6 N5 112.1(2) . .
C9 N6 H6 128(2) . .
N1 C1 H1 120.7(15) . .
N1 C1 C2 110.3(2) . .
C2 C1 H1 128.9(15) . .
C1 C2 Cl4 125.35(18) . .
C3 C2 Cl4 128.46(17) . .
C3 C2 C1 106.2(2) . .
N2 C3 C2 106.8(2) . .
N2 C3 H3 120.9(17) . .
C2 C3 H3 132.3(17) . .
N3 C4 H4A 119.7(19) . .
N3 C4 C5 110.3(2) . .
C5 C4 H4A 129.9(19) . .
C4 C5 Cl5B 125.4(3) . .
C4 C5 Cl5A 127.9(3) . .
C6 C5 Cl5B 126.5(3) . .
C6 C5 C4 106.6(2) . .
C6 C5 Cl5A 124.6(3) . .
N4 C6 C5 106.4(2) . .
N4 C6 H6A 123.2(19) . .
C5 C6 H6A 130.3(19) . .
N5 C7 H7 123.1(14) . .
N5 C7 C8 109.7(2) . .
C8 C7 H7 127.2(14) . .
C7 C8 Cl6 126.85(19) . .
C9 C8 Cl6 126.60(18) . .
C9 C8 C7 106.5(2) . .
N6 C9 C8 106.2(2) . .
N6 C9 H9 121.1(17) . .
C8 C9 H9 132.6(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 Cl1 2.3472(9) .
Cr1 Cl2 2.3228(9) .
Cr1 Cl3 2.3051(9) .
Cr1 N1 2.0781(18) .
Cr1 N3 2.1079(18) .
Cr1 N5 2.0771(18) .
CL5Bb C5 1.741(9) .
Cl4 C2 1.724(2) .
Cl6 C8 1.716(2) .
N1 N2 1.358(3) .
N1 C1 1.334(3) .
N2 H2 0.83(3) .
N2 C3 1.341(3) .
N3 N4 1.350(3) .
N3 C4 1.331(3) .
N4 H4 0.81(3) .
N4 C6 1.337(3) .
N5 N6 1.353(3) .
N5 C7 1.328(3) .
N6 H6 0.80(3) .
N6 C9 1.336(3) .
C1 H1 0.90(2) .
C1 C2 1.387(3) .
C2 C3 1.365(3) .
C3 H3 0.94(3) .
C4 H4A 0.82(3) .
C4 C5 1.384(3) .
C5 C6 1.344(3) .
C5 Cl5A 1.724(7) .
C6 H6A 0.85(3) .
C7 H7 0.91(2) .
C7 C8 1.394(3) .
C8 C9 1.363(3) .
C9 H9 0.89(3) .
